Diketene → HCID 20534014、化合物

反応式

[NH2:1][C:2]1[C:3](=[O:10])[CH:4]=[CH:5][C:6]([Cl:9])=[CH:7][CH:8]=1.[CH2:11]=[C:12]1[O:16][C:14](=[O:15])[CH2:13]1>>[Cl:9][C:6]1[CH:5]=[CH:4][C:3](=[O:10])[C:2]([NH:1][C:14](=[O:15])[CH2:13][C:12](=[O:16])[CH3:11])=[CH:8][CH:7]=1

参加物

反応物 2

HCID 12661Diketene

HCID 12557673HCID 12557673、化合物

生成物 1

HCID 20534014HCID 20534014、化合物

反応条件

温度: 100 °C

実験手順

A mixture of 2-amino-5-chloro-2,4,6-cycloheptatrien-1-one (1.55 g, described in example 9) and diketene (5 ml) were heated at 100° C. for 1 hr. The mixture was cooled and then purified by chromatography on silica gel using chloroform as the eluant. The appropriate fractions were pooled and the residue was crystallized from diethyl ether to give 650 mg of 1-[(4-chloro-7-oxo-1,3,5-cycloheptatrien-1-yl)amino]-1,3-butanedione, nmr (DMSO-d6) δ2.17 (s, 3H), 3.85 (s, 2H), 7.3 (m, 3H), 8.7 (d, 1H), 10.75 (s, 1H).

後処理

temperatureThe mixture was cooled
custompurified by chromatography on silica gel
customthe residue was crystallized from diethyl ether

出典と根拠

ORDレコード: ord-26a39316d38249cb925e9e007aff87e0
出典データセット: uspto-grants-1982_06
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US04337265

反応ノート

読み込み中…

参加物